Ruhul Kayesh

Purpose of this study was to develop a stability-indicating RP-HPLC method for routine analysis of Paracetamol (PARA), Caffeine (CAF) and Ibuprofen (IBU) in their combined solid dosage forms. The new RP-HPLC method was validated as per ICH, FDA and USP guidelines with respect to accuracy, precision, specificity, linearity, solution stability, robustness, sensitivity and system suitability. The method was developed by using a binary gradient mode of phosphate buffer (pH 7.2) and acetonitrile at a flow rate of 1.3mL/min for 15 minutes over C-18 (ODS, 150 x 4.6 mm, 5µm) column at ambient temperature. Injection volume was 20µL for both standard and sample solutions and the eluents were monitored with UV detection at 230nm.Accuracy was determined by the recovery tests of the drugs and found to be within a range of 99.89% to 100.33%. Intraday and inter-day precisions were demonstrated by a relative standard deviation being far less than maximum allowable limit (2.0%, according to FDA). The method showed linear response with a correlation coefficient (r2) value of 0.999 for all three drugs. Forced degradation studies in acidic, basic, oxidation and reduction media were carried out to establish the stability indicating tolerance of this method. Specificity was shown by the separation of drugs with high degree of resolution between them and absence of any interference from the excipients or degradation products. This method was successfully applied to assay the drugs in tablets and capsules. Hence this newly developed method can be considered suitable and reliable for the routine analysis of PARA, CAF and IBU in their solid dosage forms.

A rapid and stability indicating ion-pair reversed phase high performance liquid chromatographic method was developed for qualitative and quantitative estimation of three oxicam drugs: tenoxicam, meloxicam and lornoxicam. The method was validated according to ICH, FDA and USP guidelines with respect to accuracy, precision, specificity, linearity, solution stability, robustness, sensitivity and system suitability. The method was developed by using an isocratic condition of mobile phase comprising buffer pH 6.5 [tetra butyl ammonium hydroxide (0.008M) and sodium 1-heptane sulfonate (0.003M)] and acetonitrile in a ratio of 65:35 v/v ratio at a flow rate of 1.5 mL/min over C-18 (ODS, 250 x 4.6 mm) column at ambient temperature. The method showed linear response with correlation coefficient (r2) value of 0.999. The recoveries for all drugs were found more than 99% which demonstrated the accuracy of this method. Intraday and inter-day precision studies of the new method were less than the maximum allowable limit (RSD%£ 2.0). Forced degradation studies were carried on to check its stability indicating property. All the drugs gave sharp peaks within 7min with excellent symmetry and high resolution. Therefore, a rapid, sensitive and stability indicating ion pair RP-HPLC  method was developed for simultaneous separation of tenoxicam, meloxicam and lornoxicam in their any combination or in bulk raw materials.